CN101693790B - Composite mica cerium titanium pearl pigment and preparation method thereof - Google Patents
Composite mica cerium titanium pearl pigment and preparation method thereof Download PDFInfo
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- 239000010445 mica Substances 0.000 title claims abstract description 64
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 64
- 239000000049 pigment Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 10
- NEGBOTVLELAPNE-UHFFFAOYSA-N [Ti].[Ce] Chemical compound [Ti].[Ce] NEGBOTVLELAPNE-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 25
- 238000000576 coating method Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 150000000703 Cerium Chemical class 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 2
- 238000001556 precipitation Methods 0.000 claims 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 6
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 6
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002932 luster Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000002356 single layer Substances 0.000 abstract description 2
- 238000005253 cladding Methods 0.000 abstract 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 239000003085 diluting agent Substances 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000003608 titanium Chemical class 0.000 description 2
- -1 TiOSO 4 Chemical class 0.000 description 1
- 229910010298 TiOSO4 Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- KADRTWZQWGIUGO-UHFFFAOYSA-L oxotitanium(2+);sulfate Chemical compound [Ti+2]=O.[O-]S([O-])(=O)=O KADRTWZQWGIUGO-UHFFFAOYSA-L 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及珠光颜料技术，特别是复合型云母铈钛珠光颜料及制备方法。The invention relates to pearlescent pigment technology, in particular to composite mica-cerium-titanium pearlescent pigment and its preparation method.
背景技术 Background technique
珠光颜料在涂料、颜料、化妆品等行业应用相当普遍。CeO2-云母珠光颜料是通过液相包覆法在云母珠光颜料表面包覆氧化物CeO2，得到黄色珠光颜料，但其光泽度不够。Pearlescent pigments are widely used in coatings, pigments, cosmetics and other industries. CeO 2 -mica pearlescent pigment is coated with oxide CeO 2 on the surface of mica pearlescent pigment by liquid phase coating method to obtain yellow pearlescent pigment, but its gloss is not enough.
发明内容 Contents of the invention
本发明目的是提供光泽性好、能增加黄色CeO2-云母珠光颜料亮度的复合型云母铈钛珠光颜料及制备方法。The purpose of the invention is to provide a composite mica cerium titanium pearlescent pigment with good gloss and the brightness of the yellow CeO 2 -mica pearlescent pigment and a preparation method thereof.
本发明技术方案：复合型云母铈钛珠光颜料，包括CeO2-云母基片，在CeO2-云母基片上包覆TiO2氧化物，TiO2的包覆率为1～20％。The technical scheme of the present invention: the composite mica cerium titanium pearlescent pigment includes a CeO 2 -mica substrate, and the CeO 2 -mica substrate is coated with TiO 2 oxide, and the coating rate of TiO 2 is 1-20%.
CeO2-云母基片中CeO2的包覆率为1-50％。The coverage rate of CeO 2 in the CeO 2 -mica substrate is 1-50%.
在CeO2-云母基片上包覆TiO2氧化物的最佳包覆率为10％。The optimum coating rate of TiO 2 oxide on CeO 2 -mica substrate is 10%.
CeO2-云母基片中CeO2的最佳包覆率为30％。The optimum coverage rate of CeO 2 in the CeO 2 -mica substrate is 30%.
制备复合型云母铈钛珠光颜料的方法，按下述步骤进行：The method for preparing composite mica cerium titanium pearlescent pigment, carries out according to the following steps:
A、制备CeO2-云母基片，CeO2的包覆率为1-50％；A, prepare CeO 2 -mica substrate, the coating rate of CeO 2 is 1-50%;
B、选择可溶性钛盐，如可以选用TiOSO4、TiCl4等为Ti源。选用TiCl4时，要稀释浓TiCl4溶液，把配好的稀盐酸溶液放入冰水浴中，边搅拌边倒入液体TiCl4，TiCl4溶液浓度配制成1～30％，避光储存备用；B. Select soluble titanium salts, such as TiOSO 4 , TiCl 4 , etc., as Ti sources. When using TiCl 4 , dilute the concentrated TiCl 4 solution, put the prepared dilute hydrochloric acid solution into an ice-water bath, pour in liquid TiCl 4 while stirring, make the concentration of TiCl 4 solution 1-30%, and store it away from light for later use;
C、包覆TiO2膜层。TiO2的包覆率为1％～20％，以CeO2-云母为基片，包覆高折射率的TiO2，包覆时选择CeO2-云母基片悬浮液的浓度为1.0～20.0％，可溶性钛盐溶液浓度为0.5～20％，沉淀剂溶液浓度为0.5～1.5％，搅拌速度为50～1000r/min，水浴温度为30～95℃，pH值为1.0～4.0；C. Coating TiO 2 film layer. The coating rate of TiO 2 is 1% to 20%. CeO 2 -mica is used as the substrate, and the high refractive index TiO 2 is coated. When coating, the concentration of CeO 2 -mica substrate suspension is selected to be 1.0 to 20.0%. , the concentration of the soluble titanium salt solution is 0.5-20%, the concentration of the precipitant solution is 0.5-1.5%, the stirring speed is 50-1000r/min, the temperature of the water bath is 30-95°C, and the pH value is 1.0-4.0;
D、过滤，对包覆后的TiO2-CeO2-云母进行过滤；D, filtering, filtering the coated TiO 2 -CeO 2 -mica;
E、烘干；E. drying;
F、煅烧，煅烧温度选择700～1100℃，煅烧后得到黄色高光泽度的TiO2-CeO2-云母珠光颜料。F. Calcining. The calcining temperature is selected at 700-1100° C. After calcining, a yellow high-gloss TiO 2 -CeO 2 -mica pearlescent pigment is obtained.
制备CeO2-云母基片是以云母为基片，可溶性铈盐为铈的引入剂，以氢氧化钠、氢氧化钾、氨水、碳酸盐、尿素、草酸及可溶性草酸盐中的一种为沉淀剂，其特征是：最佳包覆条件为云母浆1～10％，NH3·H2O浓度1～5％，滴加速度1～10ml/min，搅拌速度50-1000r/min，反应温度30～95℃，pH值3.50～9.50，包覆反应完后进行过滤、烘干、煅烧得CeO2-云母珠光颜料，包覆率在1-50％时出现幻彩黄时得到的CeO2-云母珠光颜料光泽最好。The preparation of CeO 2 -mica substrate is based on mica, soluble cerium salt is the introduction agent of cerium, and one of sodium hydroxide, potassium hydroxide, ammonia water, carbonate, urea, oxalic acid and soluble oxalate is used It is a precipitant, and its characteristics are: the best coating conditions are mica pulp 1-10%, NH 3 ·H 2 O concentration 1-5%, dropping speed 1-10ml/min, stirring speed 50-1000r/min, reaction Temperature 30～95℃, pH value 3.50～9.50, filter, dry and calcinate to obtain CeO 2 -mica pearlescent pigment after coating reaction, CeO 2 obtained when magic yellow appears when coating ratio is 1-50% - Mica pearlescent pigments have the best luster.
包覆TiO2膜层使用沉淀剂为氢氧化钠、氢氧化钾、氨水、碳酸盐、尿素中的一种。The precipitating agent used for coating the TiO2 film layer is one of sodium hydroxide, potassium hydroxide, ammonia water, carbonate, and urea.
过滤后的TiO2-CeO2-云母的烘干温度为80～130℃。The drying temperature of the filtered TiO 2 -CeO 2 -mica is 80-130°C.
本发明通过多层包覆制得TiO2-CeO2-云母珠光颜料的表面光泽度比CeO2-云母珠光颜料要高得多，且CeO2-云母珠光颜料的黄色不但没有被包覆的TiO2遮盖，反而变成亮黄色，比单层包CeO2的珠光颜料光泽效果和颜色效果更好；由于光泽度高、装饰效果好，市场前景十分好，能带来丰厚的经济收益。The surface gloss of the TiO 2 -CeO 2 -mica pearlescent pigment prepared by the present invention is much higher than that of the CeO 2 -mica pearlescent pigment, and the yellow color of the CeO 2 -mica pearlescent pigment is not only without the coated TiO 2 Covering, it turns into bright yellow instead, which has better luster and color effects than single-layer CeO2 -coated pearlescent pigments; due to high gloss and good decorative effect, the market prospect is very good and can bring rich economic benefits.
具体实施方式 Detailed ways
实例1Example 1
在20％的CeO2-云母珠光颜料上包覆包覆率为20％的TiO2膜层，先包覆制得20％的CeO2-云母珠光颜料。配制稀释的TiCl4溶液备用(以下称备用稀释液)，其浓度为10％；称取20克CeO2-云母珠光颜料，加入200ml蒸馏水制得浓度为10％的CeO2-云母珠光颜料悬浮液，放在65℃的水浴中加热搅拌，搅拌速度为500r/min；取备用稀释液加入200ml的蒸馏水再次稀释浓度为10％的TiCl4溶液；配制浓度为5％的NaOH溶液500ml；先用稀盐酸把悬浮液的pH值调至3，用蠕动泵同时向CeO2-云母珠光颜料悬浮液中滴加TiCl4溶液和NaOH溶液，TiCl4溶液的滴加速度为1.3ml/min，改变NaOH溶液的滴加速度使悬浮液在65℃的水浴中保持pH值为3。当TiCl4溶液滴加完后停止反应，继续搅拌30分钟，静止2小时后洗涤过滤、烘干、900℃煅烧得到双层淡黄色珠光颜料，颜色浅黄，光泽强。The 20% CeO 2 -mica pearlescent pigment is coated with a TiO 2 film layer with a coating ratio of 20%, and the 20% CeO 2 -mica pearlescent pigment is first coated. Prepare the diluted TiCl 4 solution for subsequent use (hereinafter referred to as standby diluent), its concentration is 10%; take 20 grams of CeO 2 -mica pearlescent pigment, add 200ml distilled water to make concentration be 10% CeO 2 -mica pearlescent pigment suspension , heated and stirred in a water bath at 65°C, with a stirring speed of 500r/min; take the spare diluent and add 200ml of distilled water to dilute the TiCl 4 solution with a concentration of 10% again; prepare 500ml of NaOH solution with a concentration of 5%; Hydrochloric acid adjusts the pH value of the suspension to 3, and simultaneously adds TiCl solution and NaOH solution dropwise to the CeO 2 -mica pearlescent pigment suspension with a peristaltic pump. The rate of addition of TiCl solution is 1.3ml /min. The rate of addition was such that the suspension was kept at pH 3 in a water bath at 65°C. Stop the reaction when the TiCl 4 solution is added dropwise, continue to stir for 30 minutes, wash, filter, dry, and calcinate at 900°C to obtain a double-layer light yellow pearlescent pigment, which is light yellow in color and strong in luster.
实例2Example 2
在30％的CeO2-云母珠光颜料上包覆包覆率为10％的TiO2膜层，先包覆制得30％的CeO2-云母珠光颜料。称取10克CeO2-云母珠光颜料，加入300ml蒸馏水制得浓度为3.3％的CeO2-云母珠光颜料悬浮液，然后把悬浮液放在90℃的水浴中加热搅拌，搅拌速度为200r/min；取备用稀释液(浓度为12.8％)20.5ml加入500ml的蒸馏水再次稀释浓度为0.54％的TiCl4溶液；配制浓度为1.5％的尿素溶液800ml；先用稀盐酸把悬浮液的pH值调至2.5，用蠕动泵同时向CeO2-云母珠光颜料悬浮液中滴加TiCl4溶液和尿素溶液，TiCl4溶液的滴加速度为2.5ml/min，改变尿素溶液的滴加速度使悬浮液在90℃的水浴中保持pH值为2.5。当TiCl4溶液滴加完后停止反应，继续搅拌30分钟，静止2小时后洗涤过滤、烘干、900℃保温煅烧得到双层亮黄色珠光颜料。The 30% CeO 2 -mica pearlescent pigment is coated with a TiO 2 film layer with a coating rate of 10%, and the 30% CeO 2 -mica pearlescent pigment is prepared first. Weigh 10 grams of CeO 2 -mica pearlescent pigment, add 300ml of distilled water to prepare a CeO 2 -mica pearlescent pigment suspension with a concentration of 3.3%, then place the suspension in a water bath at 90°C for heating and stirring at a stirring speed of 200r/min Get standby diluent (concentration is 12.8%) 20.5ml and add the distilled water of 500ml to dilute concentration again and be the TiCl solution of 0.54 %; Preparation concentration is 1.5% urea solution 800ml; The pH value of suspension is adjusted to 2.5. Use a peristaltic pump to add TiCl 4 solution and urea solution to the CeO 2 -mica pearlescent pigment suspension at the same time. The dropping rate of TiCl 4 solution is 2.5ml/min. The pH was maintained at 2.5 in a water bath. Stop the reaction after the TiCl 4 solution is added dropwise, continue to stir for 30 minutes, wash and filter after standing still for 2 hours, dry, and heat-preserve and calcinate at 900°C to obtain a double-layer bright yellow pearlescent pigment.
实例3Example 3
在40％的CeO2-云母珠光颜料上包覆包覆率为5％的TiO2膜层，先包覆制得40％的CeO2-云母珠光颜料。称取10克CeO2-云母珠光颜料，加入500ml的蒸馏水制得浓度为2.0％的CeO2-云母珠光颜料悬浮液，放在60℃的水浴中加热搅拌，搅拌速度为500r/min；称取1.1g的TiOSO4固体溶解在200ml蒸馏水中制得浓度为0.55％的TiOSO4溶液；配制浓度为1％的氨水溶液500ml；先用稀盐酸把悬浮液的pH值调至3.0，用蠕动泵同时向CeO2-云母珠光颜料悬浮液滴加TiOSO4溶液和氨水溶液，TiOSO4溶液的滴定速度为0.8ml/min，改变氨水溶液的滴加速度使悬浮液在60℃的水浴中保持pH值为3.0。当TiOSO4溶液滴定完后停止反应，继续搅拌30分钟，静止2小时后洗涤过滤、烘干、900℃保温煅烧得到双层亮黄色珠光颜料，比实例2中得到的珠光颜料黄色更深。The 40% CeO 2 -mica pearlescent pigment is coated with a TiO 2 film layer with a coating ratio of 5%, and the 40% CeO 2 -mica pearlescent pigment is first coated. Weigh 10 grams of CeO2 -mica pearlescent pigment, add 500ml of distilled water to prepare a suspension of CeO2 -mica pearlescent pigment with a concentration of 2.0%, heat and stir in a water bath at 60°C, and the stirring speed is 500r/min; 1.1g of TiOSO 4 solid was dissolved in 200ml of distilled water to obtain a TiOSO 4 solution with a concentration of 0.55%; 500ml of ammonia solution with a concentration of 1% was prepared; the pH value of the suspension was adjusted to 3.0 with dilute hydrochloric acid, and a peristaltic pump was used to simultaneously Add TiOSO 4 solution and ammonia solution dropwise to the CeO 2 -mica pearlescent pigment suspension, the titration rate of TiOSO 4 solution is 0.8ml/min, change the drop rate of ammonia solution to keep the suspension at 60°C in a water bath with a pH value of 3.0 . Stop reaction when TiOSO4 solution is titrated, continue to stir for 30 minutes, wash and filter after standing for 2 hours, dry, and heat-preserve and calcinate at 900° C. to obtain double-layer bright yellow pearlescent pigment, which is darker than the pearlescent pigment yellow obtained in example 2.
实施例中所述备用稀释液指避光储存备用配制浓度成10～30％TiCl4溶液，按HCl∶H2O＝1∶5先配制稀盐酸溶液，把配好的稀盐酸溶液放入冰水浴中，边搅拌边倒入液体TiCl4而成的。The standby diluent described in the embodiment refers to the dark storage and the prepared concentration is 10-30% TiCl 4 solution, according to HCl: H 2 O = 1: 5 first prepare dilute hydrochloric acid solution, put the prepared dilute hydrochloric acid solution into ice In a water bath, pour liquid TiCl 4 while stirring.
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| CN111393875A (en) * | 2020-03-30 | 2020-07-10 | 内蒙古航天红峡化工有限公司 | Preparation method of titanium dioxide coated rare earth base pearlescent pigment |
| CN113150332B (en) * | 2021-01-23 | 2024-01-09 | 南昌诚鑫包装有限公司 | Manufacturing method of colorful pearlescent polyethylene film |
| CN116731535A (en) * | 2023-06-05 | 2023-09-12 | 瑞彩科技股份有限公司 | Preparation process of high-brightness pearlescent pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078241A (en) * | 1992-05-04 | 1993-11-10 | 广东省测试分析研究所 | The golden colour lustre pigments that rare earth is painted |
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2009
- 2009-10-22 CN CN 200910186310 patent/CN101693790B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1078241A (en) * | 1992-05-04 | 1993-11-10 | 广东省测试分析研究所 | The golden colour lustre pigments that rare earth is painted |
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| 云母钛珠光颜料及其在塑料工业中的应用;徐扬群;《塑料科技》;19970430(第2期);3-9 * |
| 制备黄色云母铈珠光颜料的工艺研究;张骞等;《江西有色金属》;20051231;第19卷(第4期);32-35 * |
| 张骞等.制备黄色云母铈珠光颜料的工艺研究.《江西有色金属》.2005,第19卷(第4期),32-35. |
| 徐扬群.云母钛珠光颜料及其在塑料工业中的应用.《塑料科技》.1997,(第2期),3-9. |
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| CN101693790A (en) | 2010-04-14 |
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